Carbon black



My 1, 1951 I 1 GHQLSQN 2,550,802

CARBON BLACK Filed Oct. 15, 1947 INVENTOR ROY L GHOLSON l-L ATTORNEYS are tworprincipaltypes: of carbonbla'ck,

Patented May 1, 1951 UNITED STATES PATENT OFFICE Ga -3222a Roy I a.GholsonsFairbanks,Lat; assignor to GolumbiamGarbon Company limitation Gctol'ier is, 19417,- SeriaI N o. 779.861

This invention relates to improvements i i-l the conversion at loose carbon black to the pelleted or'bead'ed form and provides; an improvedprocess whereby loose, floccu-lent furnace carb'o'ris may be converted to" a beaded; substantially d us-tless product having sufiicient strength to permitbulk handling and yet sufficle'r ltly friableto" permit ready dispersion in rubber;- or the like.

Carbon. blacks, as initially produced, ee xtremely light; finely divided; bulky matenah, which: readily fly intothe atmosphere;- 'I herel en the: so-called channel or? impingement blacks} and the so-called furnace blacks;-

Known means have been: developedto'r rerming free-flowing beads or pellets of channel blackof. suflicient strength to withstand shipment in large: masses, for instance, in: tank car) lo'ts,. han:- clling by mechanical'zor other. cbnveyorlsa'nd stor'-- age: in: large bins with: gravity or other: type of feed: to the point of use; Thepelleting or heading of: channel black has been developed to a). point where it is now-' common? practice to prod-11b?) so called: ,dustless channel black in: beads; or. pellets having the requisi-te'strerigth for: handlingin bulk without unduedisintegratiomot the pe'l lets or less. 015 their tree-flowing characteristics which is necessary for bulls handling; l

The use of furnace black-s by the industry is" rapidly becoming more general and: it is: highly desirable to handle blacks of this type inbulk as has been done'with the channel blacks. However, processes successful for the conversion of the flocculent channeli black tothe pelleted form have not resulted in satisfactory pelleted prod.- ucts when applied to the furnace? blacks. The

furnace blacks are; commonly converted toa:-

pell'eted form, by processes which: have beensuccessfully applied to channel blacks to in crease: their apparent density and to improve their handling characteristics: But, because of the weakness of the pellet structure produced by the application" of suchprocesses to" furnace blacks; the resultant pellets of thefurnace'bl'ackf cannot be handled by the bulk systems now use without serious" disintegration" and loss of their free-flowing characteristics? The present invention provides an: improved process for the conversion of flocculent furnacev blacks to' the pelleted form which results. in a beaded} free-flowing furnace black having the necessary strength to permit handling in bulk. The" pelleted product thus. produced has the 7 ad vantages of dustlcssness and capacity for han- 4' (llaimst (01. 23 314)" water tim or somewh a 2 l dli'ng' and shipping in bulk; characteristic of the pelleted channel blacks commonly produced. 7

As distinguished from impingem'ent blacks, the blacks herein designated furnace'black's, are; generaiiy made by lil'iriiih'g mince-arsenaina chain-f her or furnace with an amount of airiris'uilicieiit for compiete' csmtustibn and separating the re sult'arit carbon black fro'm the furnace efiluerit gases. This general ciassifieatibir also i cludes: blacks formed by thermally decomposing" hydro carbons by admixing them with hotgases, or passing tliehf contact? with highly heatd surfaces: The des-ig natibn; 'fu rnaic"e"-blacks, as used herein, a nd i theacc'ompanyihg claims; is iii-tended to include'- all blacks of the the produced 15v methodsi 'eiicludi'ri'g the so c'alled lampblacks As previously noted, it has been knewnfl'tliat the furnace bia'cks may be readily rorniedinto beads; or paints, by al gita tioii w" al'relatively small amount of water, for'i i-ista ame'unt xcfee'dingiri weight the weight at the furnace slack;- Heweven th'e resultant f inane black beads are iiagile a'hd laelc sumcient strength to withstand bulk nam oiling. The optimum proportion of watei t'd be used in forming: such: pellets varies somewhat wi thlthe'oharacteristfis ot the pafit blachusedbu inaybereadily' deter J I p1e1- test; asunderstood by the: art. Further; the optimum amount of water to be used-- With particular black; will: depend somewhat upon the type of stirring mechanism used and the vig 'cin with? which the: blackiisi stirrem For instance; more: finely divided black: will? generally require." relatively larger amounts of water. Generally, the more: dense the black: the less? water reauire'do A more dense}. smalli par ticlei sizefurnace black may requre' approximately the: same amount of water as a less dense; but coarser particle? size black-5 Also; the amoimt of water: added is: somewhat influenoed:- by the oil contentof the: black-,1 a black of higher oils. content usually requiring a larger" amount" ct: water thanv one of. smaller? oi'L content;

In: accordance: with: my present" invention;- the: furnaceblack is preliminarily subjected: to a'g'ir tationwith-an: amount of: water sufilcient to term the particular black intopellets and: thewagitaw tion .iscontinued I until fragile pellets;1 character istic of; such: treatment of furnaceblack's, are

formed. I have fOU'IIdyhQWG-VBT-y that addi integrated, and that if additional water is then added in an amount sufiicient to effect the pelleting of the entire carbon black present and the agitation continued, the composite mass of furnace black is again formed into beads, or pellets, but having substantially increased strength.

I have further found that, by repeating this procedure, furnace black pellets of adequate strength to withstand bulk handling may be formed. The procedure of forming the carbon black pellets by agitation with the water, and the subsequent disintegration of the pellets by agitating with additional dry furnace black must be repeated at least twice before furnace black pellets of adequate strength to withstandbulk handling are formed. These steps may be repeated a greater number of times, but I have found that three such pelleting operations, with intervening disruption by agitating with the additional furnace black, are usually sufficient for the purposes of the present process and that no marked advantage is normally attained by further repetition.

Predicated thereon, my present invention comprises a multi-stage process comprising the following steps:

1. A furnace carbon black is agitated with an amount of water sufilcient to form the black into pellets until the black has been substantially reduced to pelleted form.

2. Further dry furnace black is added and the agitation continued. In the process of mixing in this dry black by continued agitation the previously formed pellets are disintegrated.

3. A second increment of water is added, sufficient to form the composite black mixture into pellets, and the agitation continued until pellets are reformed.

I 4; Further dry furnace black is added and the agitation continued until the last formed pellets have been disintegrated.

' 5.A third increment of water, suflicient to form the composite mixture into pellets, is added and the agitation continued until substantiallyall of the black has been converted to pellets or beads. I

3 As previously noted, this procedure of forming the black into pellets with the subsequent disintegration f the pellets may be further repeated, but normally the three stage pelleting operation just described is adequate.

Satisfactory results are-generally more easily obtained where the black is somewhat densed, as by mechanical agitation or the like, prior to subjection to the present process. For example, the black may be deaerated by conventional means as a preliminary step to my present process. This is usually desirable, though not essential;

- It has previously been proposed in connection with the pelleting of carbon black, to agitate the black with an amount of water sufficient to form a paste. or wet plastic mass. In accordance with my present process, a'lesser amount of water is normally used; In my three stage operation, just described, I have found it particularly advantageous to add the carbon black in three substantially equal increments and further to add the water in three substantially equal increments. As previously noted, the total amount of water will vary somewhat with the particular furnace black being processed. For example, with certain furnace blacks, theoptimum total amount of water used has been found to be about 50% by weight of the carbon black, but the optimum pears from Figure 2 of the drawings.

' downcomer II is a water feed line I2.

proportions of water will be dependent on the characteristics of the particular furnace black being processed. After the final pelleting operation, the resultant pellets may be dried in the conventional manner, for instance, by heating in an oven, to drive off water.

My improved beading process will be further described and illustrated with reference to the accompanying drawings which represent conventionally and somewhat diagrammatically a small laboratory scale apparatus which has been successfully used in the carrying out of my process. It will be understood, however, that the process is' not restricted with respect to the particular apparatus employed but may be carried out in other known apparatus adapted to the thorough agitation of the materials.-

Figure 1 of the drawing is a vertical sectional view of the apparatus;

Figure 2 is a vertical transverse section alon lines 2-2 of Figure 1;

- Figure 3 is a vertical transverse section along lines 3-3 of Figure 1, and shows in particular the arrangement of an adjustable weir assembly;

Figure 4 is a further detailed view of the elements of the weir assembly;

Figure 5 is a transverse sectional view of the upper adjustable weir-extension plate; and

Figure 6 is an end view of the weir support.

The apparatus illustrated in the drawing comprises three substantially horizontal agitating chambers indicated on the drawing by the reference numerals I, 2, and 3, and herein sometimes referred to as flights I, 2, and 3. Instead of the three separate chambers, a single long chamber may be used.

Each of the flights I, 2, and 3 comprises a substantially horizontal cylindrical chamber made from 4 inches 0. D. steel boiler tubing and 29 inches in length. The flights are open on their upper sides and provided with upwardly extending flanges 4 formed by cutting the tubing along one side and turning back 1 /2 inches of the metal along each side of the cut, as more clearly ap- It is frequently desirable, especially in large scale operation, to provide a cover for these openings along the upper sides of the respective chambers, or the openings may be omitted.

Rotatably supported in each chamber is a shaft 5, supported by bearers 6 and adapted to be driven by pulley I. These shafts are inch in diameter. Extending through the shafts, and spaced apart of an inch, are a plurality of 9 inch pins 8. These pins are 3 inches long and extend an equal distance from each side of the shaft. Each pin is positioned at an angle of 45 from the pin on either side thereof so as to form a double spiral extending substantially the length of the chamber, each spiral having three complete flights over the length of the shaft.

The top chamber is provided at the extreme left with an inlet conduit 9 adapted to the introduction of dry furnace black in regulated amounts. Just to the right of conduit 9 is a water feed line I6. Extending downwardly from the extreme right of the chamber I is a downcomer II connecting the top chamber I with the intermediate chamber 2. Just to the left of the The right end of the chamber 2 is also connected with a conduit I3 adapted to the introduction of addi tional dry furnace black in regulated amounts to the chamber. Extending downwardly from the armada 5. extreme left end of chamber! and connecting that chamber with. the lower chamber 3 is downcomer l l justto the right ofwhi'ch is a water feed. line l5. Chamber 3' is also connected with conduit l6 for the introduction of additional dry furnace black in regula-tedlamounts. The right hand end of chamber 3 isconnected with conduit liT leading. to a drier, or the like not. shown.

Each of the chambers. is also provided with one or more weirs I8 shown in Figure 1 of the drawings just ahead of thedowncomers II, M, and 11, respectively. Additional. weirs, such as indicated at I8, may bepositioned atdifierent. pointsxinthe respective chambers; as subsequently herein described-.. I

the operation of my process in the apparatusshown. in the drawings, carbon black,. advan-- tageously predensed, is continuously introduced at a regulated. rate into the: upper chamber through. inlet conduit 9. Water is introduced at. a regulated rate through inlet t and the black. and. water are agitated by means of the pins. on the rotating shaft and the composite black and; water caused to move through the: chamber by reason of the spiral arrangement of the pins. Theweir I18. in chamber I is adapted to maintain the desired charge of carbon. black. in the chamber; the carbon black over-flowing past the weir and gravitating into the next lower. chamber through the downcomer I l. Addition-a1 carbon black is added at a regulated rate to chamber 2 through the conduit l3 and additional water also at a regulated rate i added through the connection The. black, is similarly. carried through the chamber 2, over Weir l8, and gravitates throughi downcomer l4 into the lower chambers 3. Additional drycarbon black is introduced to chamber 3- throughthe conduit l6 and additional water isadded through connection f. The black is carried by the spirally arranged pins through chamber flows over the weir l 8 and-passes from the chamber through conduit IT, for instance, to a drier of conventional type, not shown, but adaptedto. remove water from the pelleted carbon black. While only three flights of agitation are shown in the drawing; it will be understood' that a greater number of flights may be used where desirable.

The. arrangement. and construction of the weirs I38. are particularly shown in Figures 3, 4; 5-, and.- 6 of. the; drawings. They include a lower semi circular disc l9 notched at the middle of itsupper edge as shown to fit. substantially vertically beneath the shaft 5 so as. to. form; an obstructionacross the lower portion of the chamber. An

upper member 20 is designed, as shown, inEigure.

5 so. as to. fit, over the upper edge. of the. disc; t9. and is supported by posts 2|, extending, downwardly from bracket 22, the bracket being. designed to rest upon and be supportedby the upper edges. of. the flanges 4... The lower. ends of posts 21: are, bifurcated tofit: over. the. upper edges; of

the. disc l9 so as to support the upper portion of the; disc and. hold it in; place. The. bracket. 22 is removably tastened to flanges 4, by means not shown. The. height. ofthe. weir is. adjustable by the use of interchangeable. plates 2-0 of. variousv heights as indicated by, dotted lines in Figure 5.

Particularly advantageous results haue been obtained in. apparatu such as: describedby, add

ing; the carbon black: to the process in. three-subastantiall-y equal. incremer-ltsv through: the: conduits 9-,. l3, and i6, respectively, andadding the. water. in three equal increments through water inlets 10,. t2 and. t5, respectively. The; maximum ca 6i pacity of the. apparatus: specifically described is about ipo1mds- Ofi carbon; black; per home. The agitation shafts: are, with advantage. adapted to be operated at: variable speeds. The water ine lets: are equipped with. spray tips. of. known. type,

not; shown, adapted to operate at; a. pressure: off

from 251 to 125 pounds: per square. inch. pressure. In: a particularly advantageous: modification offthe apparatus and process just described, addi:-- tional weirs 23 and 24, of the type. described are provided. at. about; the; central; portion. ofi chambersz 2; and. 3, respectively, so. as to divide tlsiose. chambers: into two. sections. In: this method of? operation,. the; water is; introduced to the respec-- tive chambers through connections 25 and126 in:

stead. ofi through connections; I 2 and; I25; asaprevrously' described. Withathis arrangement theiupt stream half. of. the: respectire chambers. Z and; 3: serves; as; disintegrating chambers wherein: the preformed. pellets: are. broken. up by agitation. with: the. added dry furnace blacks. prior to. the addi.-- tion of; further water. Undersuclr'conditionsx of: operatiom. a; more: thorouglr. disintegration of. the? preformed pellets: is: usually more readily acc.om-=

plished'; with. resultant; improved characteristics;

isticsof the particular furnace black being processedl. The optimum: proportions of water added at' the respective points is likewise largely de-- pendent upon the characteristics of the black, including its oil content, its fineness of subdivision, its structure characteristics and the 6X tent to which the black has been predensed.

The optimum rateoffeeding. the black to the apparatus has also. been. found to vary somewhat with the characteristics; of. the particular black. andisreadily determined. by simple tests. By the used. of Weirs. so constructed, as. previously described, that their height is adjustable, theretention of. a greater or less amount of. the black. in the respective. chambers, or. sections, of. the. chambers of the apparatus is readily effected.

Also, by varying the rate: and. location of the water additions. the. size of the. pelletsmay be varied at will over a considerable range,

My process is. applicable to continuous operation in apparatus. suchas just described, or may be. carried out as. a. batch, operation, the: several steps. being, carried out. successively thesame; agitating chamber. The processis however par.- ticularly adapted to continuousoperation where.- by the several increments of furnace black. and water; respectively, are. continuously addedto the. respective agitatin zones and. the finishedbeads. are, continuously withdrawn from the finalzone.

Thefurnace black pellets formed by my proc.-,

'. Various methods have been devised for evaluat ing the bulk handling characteristics of carbon black beads, including th resistance of a single bead to crushing, mass compressibility of the beads, the resistance of the beads to bridging in flowing under pressure from a large container through a conduit of reduced size leadin from the lower end thereof, approximating conditions in a gravity feed storage bin, and the density of the pelleted black.

- The crushing characteristic of the beads is determined by placing a single bead of predetermined size on a glass microscope slide supported by one arm of an analytical balance with a second, weighted slide supported by the floor of the balance above the first slide in a plane parallel to and spaced from the plane of the first slide a distance just equal to the diameter of the bead. The other pan of the balance is then weighted by the gradual addition of measured quantities of Water" from a burette to a flask on the pan until sufficient weight has been added 'to crush the bead. This weight is then recorded in grams.

Good comparative results have thus been at-.

tained by selecting well-rounded beads of equal diameters, say, 0.6 mm.

.L-The mass compressibility of the beads is determined by using an apparatus consisting of a inch I. D. glass tube, a pair of brass plungers with platform bases and a series of weights, the plungers being of such diameter as to form a loose sliding fit within the glass tube. In carrying out the test, one of the plun-gers is inserted in the lower end of the tube, a 5 gram sample of the beads to be tested is placed in the tube and the tube is gently tapped while in a vertical position until the column of beads in the tube has come to, a constant height. The second plunger is then placed in the upper end of the tube resting on the column of beads and gradually weighed, until a total weight of 25,000 grams has been applied, the height of the bead column being measured and recorded before and after the weight is applied. From these figures, percentage mass compressibility may be calculated from the formula:

where H is the height of the column of beads before compression and H is the height of the column of beads after compression. The results of i this test have been found to be a dependable indication of the ability of the beads to retain their free-flowing characteristics under pressures such as those to which the beads are subjected in bulk handling.

The bead density is determined by weighing 100 cc. of the beads and is expressed in pounds per cubic foot.

The process will be further described and its utility illustrated by the following specific examples of its application to the beading of different furnace blacks in the previously described apparatus. In each instance, the ratio of total Water to total black used was 1:2 by weight, the black being charged in equal increments to the apparatus through conduits 9, i3, and i8 and the water being charged in equal increments at the upstream end of flight I and at intermediate points of flights 2 and 3, respectively. Also, in each instance, the flights were operated at 230 R. P. M.

EXAMPLE I A dry furnace black of low oil content (about 0.07%).Was continuously charged to the apparatus at a rate totalling 5 pounds per hour.

s": I EXAMPLE It A dry furnace black of relatively high oil content (about 1.7%) was charged to the apparatus at a total rate of 5 pounds per hour.

EXAMPLE III A dry furnace black of a type similar to that used in Example 11 was charged to the apparatus at a total rate of 5 pounds per hour.

EXAMPLE IV A dry furnace black similar to that used in Example 11 was charged to the apparatus at a total rate of 7-8 pounds per hour.

In each instance, the beads passing from flight I were quite fragile and large and were easily disintegrated by the agitation with the additional dry black in the first section of flight 2. The beads formed in the latter half of fiightZ and passing from flight 2 were likewise too fragile for bulk handling and were disintegrated in the first section of flight 3. However, the beads passing from flight 3 were well-rounded and polished and of adequate strength for bulk handling.

The mass compressibility of the unscreened beads, their density in pounds per cubic foot and the crushing strength of a 0.6 mm. bead are set forth in Table I, and the screen analysis of the beaded products of the foregoing examples are set forth in the following Table II.

Table I Mass Oom- I Crushing Sample from Example pressibmty Density Strength Lbs. per Per cent cu. ft. Grs. I 22. 5 37. 2 9.0 19. 5 38. 1 l0. 6 19. 5 39. 5 11.1 24. 0 35 7. 8

Table II Screen Analysis Per Cent on Mesh Sample from Example The foregoing test results indicate that the beads from each of the foregoing specific examples were of sufficient strength to permit their handling in bulk while capable of ready disruption and dispersion in the milling of rubber, for instance.

I claim:

1. A process for forming finely divided furnace blacks into beads adapted to bulk handling which comprises continuously passing an increment of the black and an increment of water to an agitating zone in proportions such as will form the carbon black into beads upon agitation and agitating the mixture therein until it has been substantially completely formed into beads, continuously passing the resultant beads from the agitating zone, adding a second increment of the black thereto and agitating the mixture in a second agitating zone until the beads have become disintegrated, adding a second increment of water in an amount sufficient to form the composite black mixture into beads and agitating the mixture until it has been substantially completely formed into beads, continuously passing the resultant beads from the second agitating zone, adding a third increment of the black to the beads and agitating the beads in a third agitating zone until the last formed beads have been disintegrated, adding a third increment of water in an amount sufiicient to form the composite black mixture into beads and continuing the agitation until it has been substantially completely formed into beads and continuously passing the resultant beads from the third agitating zone.

2. A process for forming furnace blacks into beads adapted to bulk handling which comprises agitating the black with an amount of water sufficient to form the black into beads until the black has been substantially completely reduced to bead form, adding to and mixing with the beads thus formed a further increment of flocculent furnace black and agitating the mixture to disintegrate the beads, adding a further increment of water to the resultant furnace black mixture in an amount sufiicient to form the composite black mixture into beads and agitating the mixture until it has been substantially completely formed into beads, adding to and mixing with the beads thus formed a further increment of flocculent furnace black and agitating the mixture to disintegrate the beads, adding a third increment of Water to the resultant furnace black mixture in an amount sufficient to form the composite black mixture into beads and agitating the mixture until beads are formed.

3. The process of claim 2 in which the water and black, respectively, are added in three equal increments.

4. The process of claim 2 in which the ratio of total water to total black is 1:2 by weight.

ROY L. GHOLSON.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 2,131,686 Heller et al Sept. 27, 1938 2,213,056 Skoog et a1. Aug. 27, 1940 2,228,704 Ofiutt Jan. 14, 1941 

1. A PROCESS FOR FORMING FINELY DIVIDED FURNAC BLACKS INTO BEADS ADAPTED TO BULK HANDLING WHICH COMPRISES CONTINUOUSLY PASSING AN INCREMENT OF THE BLACK AND AN INCREMENT OF WATER TO AN AGITATING ZONE IN PROPORTIONS SUCH AS WILL FORM THE CARBON BLACK INTO BEADS UPON AGITATION AND AGITATING THE MIXTURE THEREIN UNTIL IT HAS BEEN SUBSTANTIALLY COMPLETELY FORMED INTO BEADS, CONTINUOUSLY PASSING THE RESULTANT BEADS FROM THE AGITATING ZONE, ADDING A SECOND INCREMENT OF THE BLACK THERETO AND AGITATING THE MIXTURE IN A SECOND AGITATING ZONE UNTIL THE BEADS HAVE BECOME DISINTEGRATED, ADDING A SECOND INCREMENT OF WATER IN AN AMOUNT SUFFICIENT TO FORM THE COMPOSITE BLACK MIXTURE INTO BEADS AND AGITATING THE MIXTURE UNTIL IT HAS BEEN SUBSTANTIALLY COMPLETELY FORMED INTO BEADS, CONTINUOUSLY PASSING THE RESULTANT BEADS FROM THE SECOND AGITATING ZONE, ADDING A THIRD INCREMENT OF THE BLACK TO THE BEADS AND AGITATING THE BEADS IN A THIRD AGITATING ZONE UNTIL THE LAST FORMED BEADS HAVE BEEN DISINTEGRATED, ADDING A THIRD INCREMENT OF WATER IN AN AMOUNT SUFFICIENT TO FORM THE COMPOSITE BLACK MIXTURE INTO BEADS AND CONTINUING THE AGITATION UNTIL IT HAS BEEN SUBSTANTIALLY COMPLETELY FORMED INTO BEADS AND CONTINUOUSLY PASSING THE RESULTANT BEADS FROM THE THIRD AGITATING ZONE. 